Supercritical carbon dioxide extraction device and method

Abstract

The invention relates to the technical field of supercritical carbon dioxide extraction devices, in particular to a supercritical carbon dioxide extraction device and a method thereof.The supercritical carbon dioxide extraction device comprises a cover plate, an outer shell, a carbon dioxide tank, a pump, a recycling box, a collecting box and a pressurizing device; through dynamic stirring, modular design, partition separation, carbon dioxide recycling and a rapid operation structure, the defects that an existing supercritical carbon dioxide extraction device is low in extraction efficiency, high in maintenance cost and high in energy consumption are overcome, and the device is more competitive in industrial production; the method is suitable for large-scale extraction of the biological source inhibitor eugenol.

Description

Technical Field

[0001] The invention relates to the technical field of supercritical carbon dioxide extraction devices, and in particular to a supercritical carbon dioxide extraction device and a method thereof. Background Art

[0002] Eugenol, chemically known as 4-allyl-2-methoxyphenol, is a natural phenylpropanoid compound that is widely found in the essential oils of many plants, such as cloves, laurel, basil, etc. Its molecular structure contains phenolic hydroxyl and allyl groups, which give it antibacterial, antioxidant and anti-inflammatory biological activities. Eugenol has a significant inhibitory effect on a variety of plant pathogenic fungi (such as gray mold and anthrax) and bacteria (such as Pseudomonas syringae), and can be used to develop botanical pesticides. Eugenol can inhibit foodborne spoilage bacteria (such as Escherichia coli, Staphylococcus aureus) and fungal toxin-producing bacteria, and extend the shelf life of fruits and vegetables. As a biogenic inhibitor, eugenol has become an ideal choice to replace chemical synthetic products due to its low toxicity, biodegradability and environmental friendliness.

[0003] Common eugenol extraction methods include steam distillation, solvent extraction, supercritical carbon dioxide extraction, and cold pressing. Among them, steam distillation is to use water vapor to carry out eugenol in plant raw materials, and obtain essential oils by oil-water separation after condensation, but high temperature may destroy heat-sensitive components during extraction, resulting in partial degradation of eugenol, and low yield, high energy consumption, and is not suitable for industrial application. Solvent extraction is to use organic solvents to dissolve the eugenol components in plants, and then recover the solvent by evaporation to obtain a crude extract, but this method has a risk of solvent residues, which will affect the safety of products and the environment. Cold pressing is to directly obtain essential oils by mechanical extrusion, avoid high temperature treatment, and will not affect the safety of products and the environment, but this method has extremely low yield, is only applicable to high oil content raw materials, and cannot effectively separate eugenol from other essential oil components.

[0004] The supercritical carbon dioxide extraction method uses the high diffusivity and solubility of carbon dioxide fluid to selectively extract the target components. Its advantages are low-temperature operation, effective protection of heat-sensitive components, no solvent residue, high product purity, and suitability for large-scale production.

[0005] However, the existing supercritical carbon dioxide extraction devices have the following disadvantages: 1) The existing supercritical carbon dioxide extraction devices rely on static immersion, and the mixing effect is poor, resulting in long extraction time and low efficiency. 2) The traditional device has a fixed structure, and plant tissue or impurities can easily clog the filter plate or adhere to the inner wall of the equipment, making cleaning complicated. 3) Most of the existing devices are integrated designs, which are difficult to disassemble and have high maintenance costs. For example, the filter cartridge or inner shell cannot be disassembled, resulting in time-consuming cleaning and replacement. 4) The carbon dioxide recovery efficiency is low, and new carbon dioxide needs to be frequently replenished, which increases costs. 5) The sealing of the existing device relies on a complex fastening structure, and the operating steps are cumbersome.

[0006] Therefore, it is an urgent problem to provide a device and method for extracting eugenol with supercritical carbon dioxide which is simple to operate, has good extraction effect and is low-cost. Summary of the invention

[0007] In order to solve the above problems, the present invention provides a supercritical carbon dioxide extraction device, including a cover plate, an outer shell, a carbon dioxide tank, a pump, a recovery box, a collection box and a pressurizing device;

[0008] The inner shell, the filter cartridge and the stirring mechanism are installed on the cover plate, and the cover plate is provided with an inlet and an outlet; the bottom of the inner shell is composed of a filter plate, and the inner shell and the filter cartridge are detachably connected to the cover plate respectively, and the filter cartridge is located inside the inner shell, and the cavity between the inner shell and the filter cartridge is zone one, and the cavity between the filter cartridge and the cover plate is zone two;

[0009] The outer shell is provided with an inlet and an outlet, and a fastener is installed on the outer shell; the recovery box is provided with a liquid discharge port, and the collection box is provided with a liquid inlet, an air outlet and a liquid outlet;

[0010] The cover plate is in contact with the outer shell through fasteners, the inlet is connected to the outside and zone one respectively, the outlet is connected to zone two and the liquid inlet respectively, the air outlet is connected to the inlet of the carbon dioxide tank through a pressurizing device, the outlet of the carbon dioxide tank is connected to the inlet and outlet through a pump and valve one in turn, and the inlet and outlet are connected to the recovery box through valve two.

[0011] Preferably, the detachable connection between the inner shell body and the filter cartridge and the cover plate is a plug-in connection.

[0012] Preferably, the stirring mechanism comprises a motor and a stirring shaft, one end of the stirring shaft is connected to the output end of the motor, and the other end passes through the filter cartridge and is in contact with the filter plate, and the motor is mounted on the upper surface of the cover plate.

[0013] Preferably, a stirring rod is provided on the stirring shaft, and the stirring rod is located in zone one.

[0014] Preferably, a mounting post is installed on the cover plate, a mounting groove is provided on the outer shell, and the mounting post is placed in the mounting groove.

[0015] Preferably, a limiting block is provided on the inner surface of the outer shell, and the inner shell is in contact with and connected to the limiting block.

[0016] Preferably, the cover plate is provided with a groove, the fastener comprises a fixing seat, a bolt and a nut, the bolt is movably connected to the fixing seat, the nut is mounted on the bolt, the fixing seat is fixed to the outer surface of the housing, the bolt is placed in the groove, and the nut is in contact and connected with the upper surface of the cover plate.

[0017] Preferably, the bolt is movably connected to the fixing seat via a pin.

[0018] Preferably, a support frame is installed on the outer shell, and the support frame is connected to the ground.

[0019] The present invention has the following advantages:

[0020] (1) The present invention uses a stirring shaft and a stirring rod driven by a motor to force mixing of supercritical carbon dioxide fluid and lilac flower tissue, thereby significantly improving the mass transfer rate, solving the problem of low extraction efficiency caused by static immersion, and shortening the extraction time.

[0021] (2) The inner shell, filter cartridge and cover plate are connected by plug-in. The filter plate and filter cartridge can be quickly disassembled, which is convenient for cleaning residues or replacing parts. This solves the problem of difficult cleaning of residues and complex maintenance in traditional devices and reduces downtime.

[0022] (3) The inner shell and the filter cartridge are divided into zone one and zone two, and the filter cartridge is combined to block solid residues, ensure the purity of the extract, and improve the purity of the product.

[0023] (4) Gaseous carbon dioxide is recovered and re-liquefied through a pressurizing device for recycling, which reduces resource waste, optimizes the energy consumption of supercritical technology, and reduces production costs.

[0024] (5) Through the coordination of bolts, nuts and grooves, the cover plate and the outer shell can be quickly sealed and disassembled, which simplifies the operation process, solves the problem of cumbersome operation of traditional devices, and improves the convenience of operation.

[0025] (6) A limit block is provided inside the outer shell to fix the inner shell, and the support frame is connected to the ground to ensure stable operation of the equipment and avoid sealing failure or leakage caused by vibration of the device. BRIEF DESCRIPTION OF THE DRAWINGS

[0026] In order to more clearly illustrate the embodiments of the present invention or the technical solutions in the prior art, the drawings required for use in the embodiments or the description of the prior art will be briefly introduced below. Obviously, the drawings described below are only embodiments of the present invention. For ordinary technicians in this field, other drawings can be obtained based on the provided drawings without paying creative work.

[0027] Figure 1 This is a front cross-sectional view of the device.

[0028] Figure 2 This is a structural diagram of the cover body and the outer shell.

[0029] Figure 3 It is a top view of the cover. DETAILED DESCRIPTION

[0030] The following will be combined with the drawings in the embodiments of the present invention to clearly and completely describe the technical solutions in the embodiments of the present invention. Obviously, the described embodiments are only part of the embodiments of the present invention, not all of the embodiments. Based on the embodiments of the present invention, all other embodiments obtained by ordinary technicians in this field without making creative work are within the scope of protection of the present invention.

[0031] Example 1

[0032] A supercritical carbon dioxide extraction device and method thereof, comprising a cover plate 1, an outer shell 2, a carbon dioxide tank, a pump 4, a recovery box 5, a collection box 6 and a pressure pump 7;

[0033] The cover plate 1 is provided with an inner shell 11, a filter cartridge 12, a mounting column 15 and a stirring mechanism. The cover plate 1 is provided with an inlet 13, an outlet 14 and a groove 16. The bottom of the inner shell 11 is formed by a filter plate 1101. The inner shell 11 and the filter cartridge 12 are plug-in connected to the cover plate 1 respectively. The filter cartridge 12 is located inside the inner shell 11. The cavity between the inner shell 11 and the filter cartridge 12 is zone 18, and the cavity between the filter cartridge 12 and the cover plate 1 is zone 2 19. The stirring mechanism includes a motor 1701 and a stirring shaft 1702. One end of the stirring shaft 1702 is connected to the output end of the motor 1701, and the other end passes through the filter cartridge 12 and is in contact with the filter plate 1101. A stirring rod 1703 is provided on the stirring shaft 1702. The stirring rod 1703 is located in zone 18. The motor 1701 is installed on the upper surface of the cover plate 1.

[0034] The outer shell 2 is provided with a mounting groove 21 and an inlet and outlet 24, the inner surface of the outer shell 2 is provided with a limit block 22, and the outer surface of the outer shell 2 is provided with a fastener and a support frame 25. The fastener includes a fixing seat 2301, a bolt 2302 and a nut 2303, the bolt 2302 is movably connected to the fixing seat 2301 through a pin, the nut 2303 is installed on the bolt 2302, and the fixing seat 2301 is fixed to the outer surface of the outer shell 2.

[0035] The recovery box 5 is provided with a liquid discharge port 501 , and the collection box 6 is provided with a liquid inlet 601 , an air outlet 602 and a liquid outlet 603 .

[0036] The mounting column 15 is placed in the mounting groove 21, the inner shell 11 is in contact with the stop block 22, the bolt 2302 is placed in the groove 16, and the nut 2303 is in contact with the upper surface of the cover plate 1. The inlet 13 is connected to the outside and the zone 1 18 respectively, the outlet 13 is connected to the zone 2 19 and the liquid inlet 601 respectively, the gas outlet 602 is connected to the carbon dioxide tank inlet through the pressure pump 7, the carbon dioxide tank outlet is connected to the inlet and outlet 25 through the pump 6 and the valve 1 31 in turn, and the inlet and outlet 25 is connected to the recovery box 5 through the valve 2 502.

[0037] The working principle of this device is as follows:

[0038] The cover 1 is tightened with the outer shell 2 by the cooperation of the bolt 2302 and the nut 2303. The lilac tissue enters the zone 18 through the inlet 13. The filter plate 1101 filters out the residual liquid. At this time, the valve 2 502 is opened, the valve 1 31 is closed, and the residual liquid enters the recovery box 501 through the inlet 24. The valve 2 502 is closed, the valve 1 31 and the pump 4 are opened, and the liquid carbon dioxide in the carbon dioxide tank enters the outer shell 2 through the inlet 24, so that the liquid carbon dioxide soaks and extracts the lilac tissue. The motor 1701 is turned on to start stirring the liquid carbon dioxide and the lilac tissue to improve the extraction efficiency. The liquid carbon dioxide brings the extracted eugenol into the collection box 6. In this process, the lilac tissue is blocked by the filter cartridge 12 and remains in the zone 18. The liquid carbon dioxide enters the collection box 6 to restore the normal pressure to become gaseous and separate from the eugenol, and the pressure pump 7 is started at the same time to recover the gaseous carbon dioxide and re-pressurize and inject it into the carbon dioxide tank to achieve recovery.

[0039] After the extraction is completed, the bolts 2302 and nuts 2303 are loosened, the cover body 1 is removed, the inner shell 11 and the filter cartridge 12 are dismantled, the remaining lilac tissue is recovered, and the lilac tissue adhered to the filter plate 1101 and the filter cartridge 12 is cleaned to achieve recovery.

[0040] The above description of the disclosed embodiments enables one skilled in the art to implement or use the present invention. Various modifications to these embodiments will be apparent to one skilled in the art, and the general principles defined herein may be implemented in other embodiments without departing from the spirit or scope of the present invention. Therefore, the present invention will not be limited to the embodiments shown herein, but rather to the widest scope consistent with the principles and novel features disclosed herein.

Claims

1. A supercritical carbon dioxide extraction device, characterized in that: It includes a cover plate, an outer shell, a carbon dioxide tank, a pump, a recovery box, a collection box and a pressurizing device; The inner shell, the filter cartridge and the stirring mechanism are installed on the cover plate, and the cover plate is provided with an inlet and an outlet; the bottom of the inner shell is composed of a filter plate, and the inner shell and the filter cartridge are detachably connected to the cover plate respectively, and the filter cartridge is located inside the inner shell, and the cavity between the inner shell and the filter cartridge is zone one, and the cavity between the filter cartridge and the cover plate is zone two; The outer shell is provided with an inlet and an outlet, and a fastener is installed on the outer shell; the recovery box is provided with a liquid discharge port, and the collection box is provided with a liquid inlet, an air outlet and a liquid outlet; The cover plate is in contact with the outer shell through fasteners, the inlet is connected to the outside and zone one respectively, the outlet is connected to zone two and the liquid inlet respectively, the air outlet is connected to the inlet of the carbon dioxide tank through a pressurizing device, the outlet of the carbon dioxide tank is connected to the inlet and outlet through a pump and valve one in turn, and the inlet and outlet are connected to the recovery box through valve two.

2. A supercritical carbon dioxide extraction device according to claim 1, characterized in that: The detachable connection between the inner shell body, the filter cartridge and the cover plate is a plug-in connection.

3. A supercritical carbon dioxide extraction device according to claim 1, characterized in that: The stirring mechanism comprises a motor and a stirring shaft, one end of the stirring shaft is connected to the output end of the motor, and the other end penetrates the filter cartridge and is in contact with the filter plate. The motor is mounted on the upper surface of the cover plate.

4. A supercritical carbon dioxide extraction device and method according to claim 3, characterized in that: The stirring shaft is provided with a stirring rod, and the stirring rod is located in zone one.

5. A supercritical carbon dioxide extraction device according to claim 1, characterized in that: The cover plate is provided with a mounting post, the outer shell is provided with a mounting groove, and the mounting post is placed in the mounting groove.

6. A supercritical carbon dioxide extraction device according to claim 1, characterized in that: The outer shell has a limit block on its inner surface, and the inner shell is in contact with the limit block.

7. A supercritical carbon dioxide extraction device according to claim 1, characterized in that: The cover plate is provided with a groove, and the fastener includes a fixing seat, a bolt and a nut. The bolt is movably connected to the fixing seat, and the nut is installed on the bolt. The fixing seat is fixed to the outer surface of the housing, the bolt is placed in the groove, and the nut is in contact with the upper surface of the cover plate.

8. A supercritical carbon dioxide extraction device according to claim 7, characterized in that: The bolt is movably connected to the fixing seat via a pin.

9. A supercritical carbon dioxide extraction device according to claim 1, characterized in that: A support frame is installed on the outer shell, and the support frame is connected to the ground.

10. An extraction method using the extraction device according to any one of claims 1 to 9, characterized in that: The following steps are involved: Step 1, tighten the cover body and the outer shell by the cooperation of bolts and nuts, and the lilac tissue enters the zone 1 through the inlet; Step 2: Open valve 2, close valve 1, and the residual liquid enters the recovery box through the inlet and outlet; Step 3, close valve 2, open valve 1 and the pump, and allow the liquid carbon dioxide in the carbon dioxide tank to enter the outer shell through the inlet and outlet, so that the liquid carbon dioxide soaks and extracts the lilac flower tissue, and turn on the motor to stir the liquid carbon dioxide and the lilac flower tissue, so that the liquid carbon dioxide brings the extracted eugenol into the collection box; Step 4: Liquid carbon dioxide enters the collection box and returns to normal pressure to become gaseous and separate from eugenol. The pressurizing device is started to recover the gaseous carbon dioxide and re-pressurize it to inject it into the carbon dioxide tank; Step 5. After the extraction is completed, loosen the bolts and nuts, remove the cover, dismantle the inner shell and the filter cartridge, recover the remaining lilac tissue, and clean the lilac tissue adhered to the filter plate and the filter cartridge.

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